| 摘要 |
The invention relates to a process for developing and validating near-infrared spectroscopy and multivariate analysis methods for determining the physical properties of pharmaceutical compressed tablets. According to the invention, the process consists, in a first stage, in developing a method using calibration samples prepared according to an experimental programme, with a variable consisting of the compression force and 5...9 variation levels consisting of various values of the compression force, within the range of 5...50 kN, which are the forces at which the compressed tablets of the calibration samples are prepared, the method development being finished by achieving a multivariate calibration model able to quantisize correlations between the physical properties of compressed tables within the calibration samples and the NIR spectra thereof, followed by a second stage consisting in validating the method, using validation samples prepared according to an experimental programme with one variable and three levels, where the variable is the compression force and the levels are the various values of the compression force within the range of 5...50 kN, corresponding to 1/4, 1/ 2 and 3/4, respectively, from the values of the level scale employed upon calibration, the method being validated by comparing the values obtained through the method developed during the first stage with the values obtained through the European Pharmacopoeia methodology, while calculating the following statistic parameters: linearity, linearity range, exactness, precision and accuracy. |
